CS272264B1 - Preparation of 2,2,6,6-tetramethylpiperidilamide carboxyl saturated acids - Google Patents
Preparation of 2,2,6,6-tetramethylpiperidilamide carboxyl saturated acids Download PDFInfo
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- CS272264B1 CS272264B1 CS852720A CS272085A CS272264B1 CS 272264 B1 CS272264 B1 CS 272264B1 CS 852720 A CS852720 A CS 852720A CS 272085 A CS272085 A CS 272085A CS 272264 B1 CS272264 B1 CS 272264B1
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- tetramethylpiperidilamide
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 title claims 2
- 239000002253 acid Substances 0.000 title 1
- 150000007513 acids Chemical class 0.000 title 1
- 229920006395 saturated elastomer Polymers 0.000 title 1
- -1 2-(2',2',6',6'-tetramethyl piperid-4-yl)-propen-1-yl Chemical group 0.000 abstract 5
- 229920000642 polymer Polymers 0.000 abstract 4
- 239000004698 Polyethylene Substances 0.000 abstract 1
- 239000004743 Polypropylene Substances 0.000 abstract 1
- 239000004793 Polystyrene Substances 0.000 abstract 1
- 239000006096 absorbing agent Substances 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- 229920001155 polypropylene Polymers 0.000 abstract 1
- 229920002223 polystyrene Polymers 0.000 abstract 1
- BZSALXKCVOJCJJ-IPEMHBBOSA-N (4s)-4-[[(2s)-2-acetamido-3-methylbutanoyl]amino]-5-[[(2s)-1-[[(2s)-1-[[(2s,3r)-1-[[(2s)-1-[[(2s)-1-[[2-[[(2s)-1-amino-1-oxo-3-phenylpropan-2-yl]amino]-2-oxoethyl]amino]-5-(diaminomethylideneamino)-1-oxopentan-2-yl]amino]-1-oxopropan-2-yl]amino]-3-hydroxy Chemical compound CC(=O)N[C@@H](C(C)C)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CCCC)C(=O)N[C@@H](CCCC)C(=O)N[C@@H]([C@@H](C)O)C(=O)N[C@@H](C)C(=O)N[C@@H](CCCN=C(N)N)C(=O)NCC(=O)N[C@H](C(N)=O)CC1=CC=CC=C1 BZSALXKCVOJCJJ-IPEMHBBOSA-N 0.000 description 5
- 108700010674 N-acetylVal-Nle(7,8)- allatotropin (5-13) Proteins 0.000 description 5
- DTAFLBZLAZYRDX-UHFFFAOYSA-N OOOOOO Chemical compound OOOOOO DTAFLBZLAZYRDX-UHFFFAOYSA-N 0.000 description 1
- YAVWDJDEOLOYQO-UHFFFAOYSA-N OOOOOOOOOO Chemical compound OOOOOOOOOO YAVWDJDEOLOYQO-UHFFFAOYSA-N 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
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1 272 264
2,2,6,6-TSTPASiIETKJinKIIEPWíJIAIWH HAC£ffi£EHHHXKAPBOHOBHX KHCJIOT B KA3ECT3E CBETO-, TEPMOCTA-BOM3ATOPOB ΥΑΑΡΟΠΡΟΗΗΟΓΟ nOJIHCTJiPOJIA Ρΐ3θ6ρβΤβΗίίβ OTHOCHTCH K ΗΟΒΗΜ ΧΗΜΗ^ίθ CKHM ΟΟβ,ΙξΜΗβ-HEHM, a ΚΜΘΗΗΟ, K 2,2,6,δ-ΤβΤρβΜθΤΗΛΠΗΠθρίΙΛΗΛαΜΚΑβΜ HaCH-ΟξβΗΗΗΧ KHCJEOT, ΚΟΤΟρΗβ MOryT ΠρΜΜβΗΗΤΒΟΗ B ΚΗ^βΟΤΒθ ΟΒΘΤΟ-,TepKOCTa6HjiM3aTopoB yňaponpo^Eoro irojiorepa. Κ3ΒθστΗΗ 2,2,6,6-τθτρθΜβΤΜΛΠΗΠβρκΛΐίΛδωίΐ£Η 2,2,6,6--TeTpaMeTHjrminepííAJíJiaMJíHOKapóoHOBíiix κμολοτ, Hcno^BsyeMHeb xa^ecTBe οβθτο-, TepKOCTa6iwiíí3aTopoB πολμπροπμλθεοβογοH nOJlííaiíHAHOrO ΒΟΛΟΧΟΗ /1/.
UejrhK) HacTOflinero HsoÓpeTeutffl ηβληθτοη co3,naHne ho-BHX ΟΟθΛΗΗθΗΜΜ 2,2,6,δ-ΤβΤρθΜβΤΗΛΠΖΠΘρΖΛΙίΛΘΜΗΛΟΒ HaCMUeH-HHX KapóOHOBHX ΘΜΕΗΟΚΕΟΛΟΤ, ΚΟΤΟρΗβ MOryT ΠρΕΜβΗΕΤΒΟΕ Bxa^ecTBe βηοοκοθΦΦθκτεβηηχ οβθτο-, TepMOCTaóH^M3aTopoBy£aponpoRHoro nojrwcTíípojra. yxa3aHHafl uejih AOCTHraeTCE τθμ, eto corjiacHO Z3o6-ρθΤΘΗΗϊΟ, 2,2,&,6-ΤΘΤρβΜβΤΚΛΠΜΠβρΗΑΗΛβΜΕΑΗ XapÓOHOBHX KHC—jiot oómečt φopMyΛH:
a) npz ^3=1 η Η = 1
272 264 2 6) npz lrr> = 1 ζ η = 2 R.-NHCH2-g> -νη-0 -Ο Ό β) npH m S 2 Ζ Π = ΖΑΖ 2
κοτορειβ nojiy^ajoT Β38ΗΜ0Αθ#0ΤΒΖβΜ 4-θμζηο-2,2,6,β-τθτρβ-ΜβΤΖΑΠΜΠβρΗΑΖΗ3 (ΑΤΑΑ) C ΗΖ3ΠΙΖΜΖ θφζρβΜΖ KSpSOHOBHX KZC-jiot npz TeunepaType 160 - 210° C c οΑΗΟΒρβΜβΗΗοδ οτγοηκομBHflejisiomerocfl Hzemero cnzpTa. 2.2.6.6- τβτρ3ΜβτζΑπζπβρζΑΖΑ3ΜΖΑΗ KapČoHOBax kzcaotnpe^cTaBJíHiOT coóoií Čejiue κρζοτΒΛΑΖΜβοκζβ ποροπικζ, pacT-ΒΟρΜΜΗβ Β ÓOABIHHHCTBe ΟρΓΘΗΖΉβΟΚΖΧ paCTBOpZTeAeíí, B KK-cneicTpax npeAAaraeiáKX οοθαμηθηζ^ coAep&aTcziiojioch norAomeHza npz 1630-1685 cm” ( v? 0=0, Amza 1)3230-3390 cm”1 , Amza Π); 3405-34400 cm”1 (í jy-fj ), noATBep«flawie zx οτροβΗζβ, ΠρΜΜβρ 1. 2.2.6.6- ΤβΤρβΜβΤΖΑΠΗΠβρΖΑΖΛΘΜΖΑ UZKAOreKCZJiaMZHOyK—cycHOŽ kmcjioth (AT-12). B qeTupexropjiyio KOJtČy θμκοοτβκ) 100 ma, cHaO&eHHyioMeiuajiKOM, τβρΜΟΜβτροΜ, HacaAKOŽ Bíopna z ηζοχοαλπιημ xo-aoazabhzkom, 3arpysaioT 15,62 r (0,1 γ-μολ) ΑΤΑΑ z npznepeMemzBaHzz npzKanuBaioT 18,39 r (0,1 γ-μοα) θτζαοβογο3$zpa AZKJiorBKCMJiaMHHoyKcychoží kzcaoth. Πο OKOH^iaHzz npzKanHBaHza coAepxzMoe koa6h Harpe-BaáT ao Tewnepa^^pH 195-210° C z BHAepaczBaKT β τβτιβΗζβ1,5-2 HaCOB C ΟΑΗΟΒρΒΜβΗΗΟΚ ΟΤΓΟΗΚΟβ BHAeJIHIOIlíerOCH 3Ta-HOJia. Ilocjie οχλβ®α®ηζα ao TeanepaTypa 140° C peaKAzoHHys)Maccy 3aAHBaioT 100 ma TOAyoAa z oxAaacAaioT Ao -5 + 0° C.BHnaBmZZ npOAyKT ΟΤφΖΑΒΤρΟΒΜΒβϊΟΤ, npOMNBaiOT TOAyOAOMz cymaT. 3 272 264
Bhxoa pejieBoro npoflyKTa cocTaBjrseT 17,64 r (60 % οτTSOpeTH^teCKOrO, CHHTaH Ha 3THJI0BHÍÍ θφκρ HHKJIOreKCHJiaííHHO—yKcycHoS khcjioth), τ.πλ. 83-84° C,
SjreMeHTHHÍi cocTas: ^17^33 N3°
BhiHHCJreHO, %%'. C- 69,09, H - 11,26, N -14,23HaiUeHO, %%-. C- 68,98, H - 11,56 N -14,08 ΠρΗΜθρ 2. 2,2,6, o-TeTpaMeTKJinHnepHAHJiaidiiň MOp$ojiHHoyKcycHOiíkhcjioth (AT-13). AHajrorHHEO npHMepy 1, H3 15,62 (0,1 γ-moji) ATAA h17,28 r (0,1 r—moji) sTKJiOBoro 3<£npa Mop$ojiHHoyKcycHoS khc-jioth nojiynaioT 14,9 r (52,6 % οτ τβορβτκπβοκογο, cwaa Ha3Thjiobh^ οφπρ Mop<£ojiíiHoyKcycHoS khcjioth) 2,2,6,6- TeTpa-MeTHJiniinepHflKjraMHAa MOp$ojiHHoyKcyCHoS khcjioth c T.nji.103-104° C (TOJiyoji). N3°2 10,31, N - 14,8310,28, N - 14,48 ΠρΗΜβρ 3. 2,2,6,δ-ΤβΤρβΜβΤΗΛΠΗΠβρΗΑΗΛΘΜΗΑ IIHnepHflHHOyKCyCHOMkhcjioth (AT-14). AHaJiornnHOMy npHMepy 1, H3 62,48 r (0,4 γ-moji) ATAAh 68,34 r (0,4 r—moji) 3THjroBoro 3$npa nHnepHAHHoyKeycHOžíkhcjioth nojiynaBT 94,2 r (80,6 % οτ TeopeTHHecKoro,CHHTaHHa 3THJT0BHH βφκρ nKnepH£HHoyKcycHofó khcjioth) nejieBoro npo-ňyKTa c T.nji. 76-78° C. 3° 11,10, N - "4,9310,91 N - 14,83 aHHJIHHyKCyCHOH KHCJIO- cocTaB: C^gHgg C 63,57, H -C 63-74, H -
SjíeueHTHHH BHHHCJieHO,Han^eHO, %%: BHHHCJieHO,
HaítneHo, ΠρΗΜβρ 4. 2,2,6,6-TeTpaMeTHjinHnepHAHJiaMHíi
SjíeMeHTHHH cocTaBí C16H31 C - 68,28,C - 68,61, τη (AT-15). 272 264 4 AHaJiorH^HO npHMepy 1, η3 23,44 (0,15 γ-moji) ATAA η26,7 Γ (0,15 Γ-MOJl) 3ΤΗΛ0Β0Γ0 ΟφΜρ^ aHMJIMHOyKCyCHOM KMC-λοτη nojiynaioT 41,3 r (82,17.% οτ τβορβτκΗβοκοΓΟ c^MTaa Haθτηαοβημ θφπρ aHHAMHoyKcycHoií kmcjioth) β,θ,λθβογο npoAyKTac ®. ΠΛ. 173-174° C (M3O-nponaHOA). Θλθμθητηημ cocTaB: C17H27 ν30 -11,06, -11,68 BOTHCJieHO, %%: C - 70,55, Η - 9,40,
HatoHO, %%: C - 70,34, Η - 9,96, ΠριίΜθρ 5. Ν, Ν — Bhc- (2,2,6,6-TeTpaMeTHjinHnepiíflMJi)-aiíeTa-mha nBnepa3HHa (AT-16). Αηηαογηήηο npHMepy 1, hs 31,35 r (0,2 γ-moji) ATAAh 25,75 r (0,1 r—moji) αμοτηλοβογο 3$wpa nnnepasHHOAHyKcychojí kmcjioth nojiynaiOT 37 r (77,08 % οτ τβορβτκΗβοκοΓΟ, chh·Taa Ha stmjiobhh 3$np nMnepa3MH0AHyKcycH0H kmcjioth) nejie-βογο npoAyKTa c t. na. 230-230,5° C (TOJiyoji). 3jieweHTHHŽí cocTaB: C26H50 N 6θ2 C - 65,23,C - 65,30, H - 10,52H - 10,60, - 17,55, - 17,78
BaujicjieHo, %%:
HaMASHO, %%·. ΠρΗΜβρ 6. 2,2,6,6-TeTpaweTMJinMnepnAMJiaMMA, AHKJioreKCMJiaMMHO-npOIMOHOBOÍÍ KMCJIOTH (AT-30). AHajiorwBHO npHMepy 1, M3 34,38 r (0,22 γ-moji) ATAAH 37,05 Γ (2 Γ-MOJI) MeTHJIOBOrO 3$Mpa AMKJIOreKCHJiaMHHO-προ·nnoHOBoS kmcjioth npn TennepaType 170-185° Ο b TeneHne3 qacoB no.ayqaioT 26,7 r (43,2 % οτ TeopeTM^ecKoro, cHMTaaHa MeTMJIOBHIl 3φπρ AHKJIOreKCHJiaMMHOnponMOHOBOČí kmcjioth)ΑΘΛβΒΟΓΟ npoAyKTa c t.iui. 121-123° C. Βλθμθητηημ cocTaB: C18H35 BHMMCJieHO,Haleno, %%·. 0 - 69,55,C - 69,85 N 30 H - 11,32,H - 11,4, N - 13,43,N - 13,58 5 272 264 ΠρκΜβρ 7. Ν,Ν^ -ČHC- ( 2,2,6,6~ΤδΤρ£ΙίΛβΤΜΛΠΜΠβρΗΑΗ·3)-Πρ0ΠΗ0-HaMMfl nnnepa3MHa (AT-31).
AnajiorHHHO npmíepy 6, na 25,8 (0,1 γ-moji) αημθτηλο-ΒΟΓΟ scpupa nMnepa3MHO,HíinponHOHOBOM KHCJIOTH H 34,38 Γ(0,22 γ-moji) ATAA nojryqaioT 17,2 r (33,94 % ot TeopeTjmec-ΚΟΓΟ, CHHTaH Ha flHMeTHJIOBHH 3φκρ ΠΜΠερββΖΗΟΛΗΠρΟΠΗΟΗΟΒΟΗ khcjioth) uejreBoro npo^yKTa c T.nji. 160-162OjreiáeHTHiáS cocTaB: C. C28H54 6°2 C - 66,64,C - 66,36, H - 10,71H - 10,74 - 16,01- 16,58 BHHHCJieHO,
HaitASHO, npHMep 8. 2,2,6,6-TeTpaweTHjinKnepH£JiJiaMK£ 6eH3MJiaMHHonpnMO-hoboh khcjioth (AT-32). AHajrorHTOO npHMepy 6, H3 57,99 r (0,3 γ-moji) μθτη-ΛΟΒΟΓΟ 3$íipa 6eH3HJiaMHHOnpon5IOHOBO2 KHCJIOTH H 50,00 Γ(0,32 r—moji) ATAA noJiynaioT 53,77 r (51,2 % ot TeopeTHnec-ΚΟΓΟ, CHHTaa Ha MeTHJIOBHŽ θφκρ 6eH3HJiaMHHOnponMOHOBOft KHC-jtoth) pejieBoro npoňyKTa c T.nji. 132-134° C. 3Jieaiehthhh cocTaB: Ηθ^ ΝθΟ
SsraicjieHO, C - 70,92, H - 9,68, N - 13,71
HaiUeHO, %%: C - 71,81, H - 9,84, N - 13,24
HpHMep 9. 2,2,6,6, -TeTpaMeTHjrnHiiepH.ZíiíjraMHA N -μ ορφΟΛΗΗΟπρο-HHOHOBOÍÍ KHCJIOTH (AT-33). ÁHajiorHHHo npHMepy 6, H3 17,32 r (0,1 γ-moji) μθτηπο-ΒΟΓΟ θφκρβ N -MOpφOJIHHOΠpOΠHOHOBO$í KHCJIOTH H 17,19 Γ(0,11 γ-moji) A^AA nojiyqaioT 13,5 r (45,4 % ot ΤθορθτκΗθοκο—Γ0, CHHTaH Ha MeTHJIOBHS 3φκρ N -MOpφOJIHHOΠpOΠHOHOBOδ KHC“jioth) HejieBoro npoflyKTa c T.nji. 82-83° 0. C16 H31 n 3°2 64,52, H - 10,72, N - 14,29 64,61, H - 10,50, N - 14,13 oJieMeHTHHH COCTaB: C -C - BHHHCJieHO,ΗΗΚΑβΗΟ, %%: 272 264 6 IIpHiiep 10. 2,2,6,6-TeTpaMeT5iJinMnepHAiiJiaMMfl N -nznepzAMHonpo-ΠΜΟΗΟΒΟΜ KHCHOTEI (AT-34) . Αηηλογμ^ηο npMMepy 6, H3 34,24 r (0,2 γ-μολ) μθτμ-ΠΟΒΟΓΟ 3$npa N -ΠΜΠθρΗΑΗΗΟΠρΟΠΗΟΗΟΒΟίί KMCJIOTH H 34,33 Γ(0,22 γ-μολ) ATAA nojiynaioT 29,3 r (49,6 % ot TeopeTH-qeο-κογο, ΟΗΗΤΗΗ Ha ΜΘΤΚΛΟΒΗίί οφκρ -ΠΚΠβρΜΑΖΗΟΠροΠΗΟΗΟΒΟδkmcjiotn) iíejieBoro npoflyKTa c τ,πλ. 133-134° C. 3jieMeHTHnií cocTaB: C17H 33N3°2 Βηημοηθηο, %%·. 0 -. 69,47, H - 11,84, N - 14,63
Haleno, %%: C - 69,10, H - 11,26, N - 14,22 Πρκωθρ 11. Ροτοβητ κοΜπο3ζΐξΐιιο, cocToamym ks yflaponponHoro πο-HHCTjapojia c soSaBKOŽ 0,5 Mac.q. CTaČHJiHSaTopOB. PÍ 3 nojiy-ΗβΕΗΗΧ ΚΟΜΠΟβκυ,Ηβ ΓΟΤΟΒΗΤ 5 % Č6H3 OJIbHBIM paCTBOp. IlOCJieποληογο pacTBopeHHH nojiKMepa h cTa6njiM3aTOpa b 6θη30λθμθτολομ nojiHBa Ha H,ejiJio$aHOByK) nojmosney, orpaHHqeHHy©CTeKJIHHHHM KpyrOM, OTJIHBaiOT ΠΛ6ΗΚΖ. 4ΛΗ CpaBHeHMH ΓΟΤΟΒΗΤ aHanOrHqHLie Κ0ΜΠ03ΗΓξΗΜ C TH —HyBHHOM Π, a τβκκθ ΠΛθΗκκ noHHMepa óes cTa6nHH3aTopa.IIojiyqeHHhie πλβηκμ τολπϊμηοΓι 70 mkm oÓJiywaKT ΗθφϋΛΒτροΒβΗ-HHM yJIbTpaφHOJIeTOBδIM ΟΒΘΤΟΜ B Ορβββ B03AyXa. B npoijecce cTapeHMH oTózpafflT προδΗ μ οπρβ,ξβΛΗωτ οτθ- neHb ΛθΟΤρνΚΙίΗΜ ΠΟΛΗΜθρβ ΜΘΤΟΑΟΜ ΜΚ-ΟΠβΚΤρΟΟΚΟΠΗΗ ΠΟ Ηθ- -1 κοπλθηηιο KapÓOHKHbHHX rpyiin Β οδΛβοτζ 1600-1800 CM ΗcoxpaHeHHK) κολμηθοτβθ aboííhiíx CBH3eíí b οΡληοτη 800-1000 cmb npopecce yΛbτpaφiIOΛeτoBOΓO oójryqeHWH.
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S 33 03 272 264 8 K3 AaHHHXj ΠρίΙΒβΛβΗΗΗΧ Β ΤβδΛΗΙξβ 1, ΒΜΑΗΟ, ηΤΟ ΒΟβMccjieflOBaHHbie οοθαμηθημη hbjíhktcíi cBeTocTaÓHJiHsaTopaMHyAaponpoHHoro nojincTMpojia.
Bhcokoíí cBeTocTačHJiiisHpyiomeíí θΦΦθκτμβηοοτβιο očjia^aioTοοβΛΗΗθΗΗΗ AT-34, AT-15, AT-14, AT-16, AT-33, AT-30,κοτοριίθ b '"•s 1,5 pa3a npeBCcxoAHT TZHyBMH Π.
CoeflMHeHne AT-31 no cBeTocTa6njrn3Mpyiomei5 θφφβκτΗΒΗΟ-ctm HaxoflHTCH Ha ypoBHe TMHysHHa Π, a οοβαμηθημη AT-12,AT-13, AT-32 ΗΘΟΚΟΛΒΚΟ npeBOCXOflHT no ΘφφβΚΤΜΒΗΟΟΤΚ THHy-BMH Π.
IlpuMep 12. OCpaaiíH παθηοκ yAaponpo^Horo nojizcTnpojia b npucyTCT—bmm 0,5 Mac.H. cTaÓHjinsaTopOB γοτοβητ no MeTOAy, yKasan-Howy b npwMepe 1. Rjui ορθβηθημη γοτοβητ aHajiorz^HHe kom-πο3μβ;μμ c nojmrapfiOM η πλθκκμ m3 HecTa6HJiM3MpoBaHHoro no-jiMMepa. ΠΛθΗΚΜ TOJinWHOČÍ 70 MKM ΠΟβΒβρΓΘΕΤ ΤβρΜΟΟΤβρβΗΗΙΟ npMTe^nepaType 120° C b cpe#e Bosflyxa c nocjreAyíomHM οτδοροΜπρού μ CHflTneM ΚΚ-οπβκτροΒ norjioineHHH β očjiacTH 1600-1900 cmμ β oóJiacTH 900-1000 cm-1. IIojiy^eHHHe αθηηηθ πρΜΒβΑθΗϋ β TaČJisme 2. H3 flaHHHX, ΠρΚΒβΑβΕΗΚΧ B TaÓJUÍIje 2, Β ΜΑΗ o, η TO BceHccjieAOBaHHbie οοθαμηθημη hbjihiotch TepMOCTačMAKsaTopaiíJíyAaponpOHHoro nojMCTMpoAa, 3HaHHTejtbH0 npeBocxoAflmne noθφφθΚΤΜΒΗΟΟΤΜ IlOJIHrapA·
Bhcokmm TepMOCTaÓHJiH3MpyioiiiiHM θφφβκτοΜ o6jraAas>T coe-Αμηθημη AT-15, AT-16. HecKOJibKO mm ycTynaioT no θφφθκτκΒ-HOCTM ΟΟΘΑΜΗΘΗΜΗ AT-32, AT-33, AT-34, AT-12 κ ββτβΜ οοθαη—ΗβΗΗΑ AT-30, AT-13, AT-14.
JlHUIb ΟΟθΑΜΗΘΗΜβ AT-31 ΠΟ TepMOCTatíMAHSHpyiOiqeŽ θφφθΚΤΗΒ-hocth ycTynaeT βοθμ μοολθαοβθηημμ οοθαμηθημημ μ ηθχοαητοηna ypoBHe nojnirapAa. 9 272 264 R CO « R R « R O • CO • CD i S2 05 Ol R CO CO R a a*a čřs Jl> > > > > > > > > > a a a o E H H H i-3 1-3 I 1-3 1 1-3 1 1-3 J o b X Φx o Γ3 Φ O4 CO co 00 co 00 R R R R R s X *3 σι a R 00 co R o 05 Ol R CO CO a X SC X Sc Ol Λ a a a b fa a a X a »3 a o a a o I X R R R R R R R R R R R R o O O O O O O O O O O O O a a φ t~R t-U s X R R R R R M R M R R w R M R w R Ol w R O a X o O R CO 05 co O o 05 S2 -3 00 05 O o »3 a fa X φ a X R R R CO R R R CO CO CO 05 05 CO o φ X a φ cn R ^2 <O -0 CO 05 R ω R CO R . o a X o II CO CO CO R Ml CO m CO w CO CO w co CO w 05 w a fa co o o CO 05 CD co o 05 co R -0 R 05 φ X o X X a X o a X «< CO CO CO a t* R CO w co R w R w R w a x 3 R O a a -0 on Ol φ R -o o R R R φ O O X X a X X a 5B X X R *« R R *· 3 CD w CD w co «« R Ol R w a fa X Ol O R o to O o R o co R 05 o o O a a X o ω R R R © fa Oi co ω Ol Ol R X fa 05 w © w M- w X o R o co O o co co co 05 05 o o X X R R R R R R R R R R R R o o O O O O O O O O O O O O O O O O O O O O O O O R R R R R R R R a o o O O O O O CO co CO rf* CO O O O O O O O O co R 05 R a o a φ Cd o s b R co X Φ CD <O CD <2 CD co O CD S2 00 CO co o a CD 00 CO O Ol CO O CO CO CD 05 co o O s 03 X X a a σ> <2 05 CO O. 05 05 <2 05 <2 co a co φ φ O CO O CO R o CD O CO Ol o fa φ o o A s Ω a X a X II tn R R a fa R R Ol Ol R Ol fa φ X R Ω R O Ό φ X O CO co O CO Ol X X a o O o X 1 s X a X 03 a o O a X a R R R X CO R R R co R o fa Ol řG CO Ό R o a co Ol 05 R R 05 a a X o o o a X X X X fa fa X CO R CD X CO CO CO ω CO CO o 05 σ> SJ -3 o X Ol OD CO co 00 CO X o o o o a ' •3 a x X X Xσι a oa φ afa acfa * s φ O x-s a X ÍŘS i3 φ O O a *3 X o X a aa o Ol a x O o a 3b a a a fa o o a js a a Φ o a O "S X o φ a a a >3 φ fa a a φ a 2 a o X o X o »3 X •3 X a a«< o φ b o a x a a a •3 X o Φ a fa >~a X »3 O a Φ X a 2 a φ a oφ a φa o b© sa a a
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1,272,264
,6 θ ΧΗΜΗ AC ,6 ,6 ,6 ,6 ,6 í ,6 AC AC AC AC AC AC AC AC AC AC AC AC AC AC AC AC EH EH EH EH EH CHρΤρβΜθΤΗΛΠΗΠθρίΙΛΗΛαΜΚΑβΜ HaCH-ΟξβΗΗΗΧ KHCJEOT, ryρΗβ MOryT ΠρΜΜβΗΗΤΒΟΗ B ΚΗ ^ β yθ ΟΒΘΤΟ-, TepKOCTa6HjiM3aTopoB ynaponpo ^ Eoro irojiorepa. Κ3ΒθστΗΗ 2,2,6,6-τθτρθΜβΤΜΛΠΗΠβρκΛΐίΛδωίΐ £ Η 2,2,6,6 - TeTpaMeTHjrminepííAJíJiaMJíHOKapóoHOBíiix κμολοτ, Hcno BsyeMHeb ^ x ^ ecTBe οβθτο-, TepKOCTa6iwiíí3aTopoB πολμπροπμλθεοβογοH nOJlííaiíHAHOrO ΒΟΛΟΧΟΗ / 1 /.
UejrhK) HacTOflinero HsoÓpeTeutffl ηβληθτοη CO3 tips it ΟΟθΛΗΗθΗΜΜ BHX-2,2,6, δ-ΤβΤρθΜβΤΗΛΠΖΠΘρΖΛΙίΛΘΜΗΛΟΒ HaCMUeH HHX-KapóOHOBHX ΘΜΕΗΟΚΕΟΛΟΤ, ΚΟΤΟρΗβ Ballad ΠρΕΜβΗΕΤΒΟΕ BXA-ecTBe βηοοκοθΦΦθκτεβηηχ οβθτο-, TepMOCTaóH M3aTopoBy ^ £ aponpoRHoro nojrwcTíípojra. yxa3aHHafl uejih AOCTHraeTCE τθμ, eto corjiacHO Z3o6-ρθΤΘΗΗϊΟ, 2,2, &, 6-ΤΘΤρβΜβΤΚΛΠΜΠβρΗΑΗΛβΜΕΑΗ XapÓOHOBHX KHC — jiot oómečt φopMyΛH:
a) npz ^ 3 = 1 η Η = 1
272 264 2 6) npz lrr> = 1 η η = 2 R.-NHCH 2 -g> -νη-0 -Ο Ό β) npH m S 2 Π Π = ΖΑΖ 2
κοτορειβ nojiy ^ ajoT Β38ΗΜ0Αθ # 0ΤΒΖβΜ 4-θμζηο-2,2,6, β-τθτρβ-ΜβΤΖΑΠΜΠβρΗΑΖΗ3 (ΑΤΑΑ) C ΗΖ3ΠΙΖΜΖ θφζρβΜΖ KSpSOHOBHX KZC-jiot npz TeunepaType 160-210 ° C c οΑΗΟΒρβΜβΗΗοδ οτγοηκομBHflejisiomerocfl Hzemero cnzpTa. 2.2.6.6- τβτρ3ΜβτζΑπζπβρζΑΖΑ3ΜΖΑΗ KapČoHOBax kzcaotnpe ^ cTaBJíHiOT coóoií Čejiue κρζοτΒΛΑΖΜβοκζβ ποροπικζ, pACT-ΒΟρΜΜΗβ Β ÓOABIHHHCTBe ΟρΓΘΗΖΉβΟΚΖΧ paCTBOpZTeAeíí B KK-cneicTpax npeAAaraeiáKX οοθαμηθηζ coAep ^ & aTcziiojioch norAomeHza NPZ 1630-1685 cm '(v? 0 = 0, Amza 1) 3230 -3390 cm ”1, Amza Π); 3405-34400 cm ”1 (i-j), noATBep« flawie zx οτροβΗζβ, ΠρΠβρ 1. 2.2.6.6- ΤβΤρβΜβΤΖΑΠΗΠβρΖΑΖΛΘΜΖΑ UZKAOreKCZJiaMZHOyK — cychoK kmcjioth (AT-12). B qeTupexropjiyio KOJtČy θμκοοτβκ) 100 mA, Chao & eHHyioMeiuajiKOM, τβρΜΟΜβτροΜ, HacaAKOŽ Bíopna from ηζοχοαλπιημ oxo-aoazabhzkom, 3arpysaioT 15.62 r (0.1-γ μολ) ΑΤΑΑ of npznepeMemzBaHzz npzKanuBaioT 18.39 r (0.1-γ μοα ) θτζαοβογο3 $ zpa AZKJiorBKCMJiaMHHoyKcychoží kzcaoth. Pe O ο p p p p pe pe pe pe pe pe pe pe pe pe pe pe pe pe pe 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 195 HA HA HA HA HA HA HA HA HA B B B. Ilocjie οχλβ®α®ηζα and TeanepaTypes 140 ° C peaKAzoHHys) Maccy 3aAHBaioT 100m and TOAyoAa from oxAaacAaioT Ao -5 + 0 ° C.BHnaBmZZ npOAyKT ΟΤφΖΑΒΤρΟΒΜΒβϊΟΤ, npOMNBaiOT TOAyOAOMz cymaT. 3,272,264
Bhxoa pejieBoro npoflyKTa cocTaBjrseT 17.64 r (60% οτTSOpeTH ^ teCKOrO, CHHTaH Ha 3THJI0BHIÍ θφκρ HHKJIOreKCHJiaííHHO — yKcycHoS khcjioth), τ.πλ. 83-84 ° C
SjreMeHTHIi cocTas: ^ 17 ^ 33 N3 °
BhiHHCJreho, %% '. C-69.09, H-11.26, N -14.23HaUeHO, %% -. C- 68.98, H - 11.56 N -14.08 ΠρΗΜθρ 2. 2,2,6, o-TeTpaMeTKJinHnepHAHJiaidium MOp $ ojiHHoyKcycHOhqjioth (AT-13). AHajrorHHEO npHMepy 1, H3 15.62 (0.1 γ-my) ATAA h17.28 r (0.1 r — my) sTKJiOBoro 3 <£ npa Mop $ ojiHHoyKcycHoS khc-jioth nojiynaioT 14.9 r (52.6% οτ τβορβτκπβοκογο, cwaa Ha3Thjiobh ^ οφπρ Mop £ j j K K K K K K K K K K ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 ,6 oy oy 4 (((((TO TO TO N3 ° 2 10.31, N - 14.8310.28, N - 14.48 ΠρΠβρ 3. 2,2,6, δ-ΤβΤρβΜβΤΗΛΠΗΠβρΗΑΗΛΘΜΗΑ IIHnepHflHHOyKCyCHOMkhcjioth (AT-14). AHaJiornnHOMy npHMepy 1, H3 62.48 r (0.4 γ-moji) ATAAh 68.34 r (0.4 r — my) 3THjroBoro 3 $ npa nHnepHAHHoyKeycHeichhkjioth nojiynaBT 94.2 r (80.6% οτ TeopeTHHecKoro, CHHTaHHa 3THJT0BHH βφκρ nKnepH H HHoyKcycHofó khcjioth) nejnoBoro npo-KT kaca c T.nji. 76-78 ° C. 3 ° 11.10, N - "4.9310.91 N - 14.83 and HH 1 HHYKCyCHOH KHCJ 10 - cocTaB: C C gHg C 63.57, H -C 63-74, H -
SjíeueHTHHH BHHHCJieHO, Han ^ eHO, %%: BHHHCJieHO,
HaitneHo, ΠρΗΜβρ 4. 2,2,6,6-TeTpaMeTHjinHnepHAHJiaMHi
<RTIgt; Cl6H31C-68.28, </RTI> C-68.61, tη (AT-15). 272 264 4 AHaJiorH ^ HO npHMepy 1, η3 23,44 (0,15 γ-my) ATAA η26,7 Γ (0,15 Γ-MOJl) 3ΤΗΛ0Β0Γ0 ΟφΜρ ^ aHMJIMHOyKCyCHOM KMC-λοτη nojiynaioT 41,3 r (82,17 .% οτ τβορβτκΗβοκοΓΟ c ^ MTaa Haθτηαοβημ θφπρ aHHAMHoyKcycHoii kmcjioth) β, θ, λθβογο npoAyKTac ®. ΠΛ. 173-174 ° C (M 3 O-nponaHOA). Ocλθμθητηημ cocTaB: C17H27 ν30 -11.06, -11.68 BOTHCJieHO, %%: C - 70.55, Η - 9.40,
HatoHO, %%: C - 70,34, Η - 9,96, ΠριίΜθρ 5. Ν, Ν - Bhc- (2,2,6,6-TeTpaMeTHjinHnepiflMJi) -aiTa-mha nBnepa3HHa (AT-16). Αηηαογηήηο npHMepy 1, hs 31,35 r (0,2 γ-moji) ATAAh 25,75 r (0,1 r — my) αμοτηλοβογο 3 $ wpa nnnepasHHOAHyKcychojí kmcjioth nojiynaiOT 37 r (77,08% οτ τβορβτκΗβοκοΓΟ, chh · taa Ha stmjiobhh 3 $ np nMnepa3MH0AHyKcycH0H kmcjioth) nejie-βογο npoAyKTa c t. 230-230.5 ° C (TOJiyoji). 3jieweHTHZi cocTaB: C26H50N 6θ2C - 65.23, C - 65.30, H - 10.52H - 10.60, - 17.55, - 17.78
BaujicjieHo, %%:
HaMASHO, %% ·. ΠρΗΜβρ 6. 2,2,6,6-TeTpaweTMJinMnepnAMJiaMMA, AHKJioreKCMJiaMMHO-npOIMOHOBOi KMCJIOTH (AT-30). AHajiorwBHO npHMepy 1, M3 34.38 r (0.22 γ-moji) ATAAH 37.05 Γ (2 Γ-MY) MeTHJIOBOrO 3 $ Mpa AMKJIOreKCHJiaMHHO-προ · nnoHOBoS kmcjioth npn TennepaType 170-185 ° Ο b TeneHne3 qacoB no. ayqaioT 26.7 r (43.2% οτ TeopeTM ^ ecKoro, cHMTaaHa MeTMJIOBHIl 3φπρ AHKJIOreKCHJiaMMHOnponMOHOBOČi kmcjioth) ΑΘΛβΒΟΓΟ npoAyKTa c t.iui. 121-123 ° C. CocTaB: C18H35 BHMMCJieHO, Haleno, %% ·. 0 - 69,55, C - 69,85 N 30 H - 11,32, H - 11,4, N - 13,43, N - 13,58 5,272,264 ΠρκΜβρ 7. Ν, Ν ^ -ČHC- ( 2,2,6,6 ~ ΤδΤρ £ ΙίΛβΤΜΛΠΜΠβρΗΑΗ · 3) -Πρ0ΠΗ0-HaMMfl nnnepa3MHa (AT-31).
AnajiorHHHO npmiepy 6, to 25,8 (0,1 γ-moji) α-p scpupa nMnepa3MHO, HíinponHOHOBOM KHCJIOTH H 34,38 Γ (0,22 γ-moji) ATAA nojryqaioT 17,2 r (33,94% ot TeopeTjmec -ΚΟΓΟ, CHHTaH Ha flHMeTHJIOBHH 3φκρ ΠΜΠερββΖΗΟΛΗΠρΟΠΗΟΗΟΒΟΗ khcjioth) uejreBoro npo ^ yKTa c T.nji. C-C28H54 6 ° C -66.64, C-66.36, H-10.71H-10.74-16.01- 16.58 BHHHCJieHO,
HaitASHO, npHMep 8. 2,2,6,6-TeTpaweTHjinKnepHiJiaMK-6eH3MJiaMHHonpnMO-hoboh khcjioth (AT-32). AHajrorHTOO npHMepy 6, H3 57.99 r (0.3 γ-moji) θ 3 $ íipa 6eH3HJiaMHHOnpon5IOHOBO2 KHCJIOTH H 50.00 Γ (0.32 r — my) ATAA noJiynaioT 53.77 r (51.2% ot TeopeTHnec-ΚΟΓΟ, CHHTaa Ha MeTHJIOBHŽ θφκρ 6eH3HJiaMHHOnponMOHOBOft KHC-jtoth) pejieBoro nvomyKTa c T.nji. 132-134 ° C. 3Jieaiehthhh cocTaB: Ηθ ^ ΝθΟ
SsraicjieHO, C-70.92, H-9.68, N-13.71
HaiUeHO, C = 71.81, H-9.84, N-13.24
HpHMep 9. 2,2,6,6, -TeTpaMeTHiOnHiPiOnHiOnHiOnNHeOnHnOnHHOHOBOiHe KHCJIOTH (AT-33). HHajiorHHHo npHMepy 6, H3 17.32 r (0.1 γ-moji) θ θ θ------^ ^ ^ ^ ^ ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 ,5 , 4% ot —θορθτκΗθοκο — Γ0, CHHTaH Ha MeTHJIOBHS 3φκρ N -MOpφOJIHHOΠpOΠHOHOBOδ KHC “jioth) HejieBoro npoflyKTa c T.nji. 82-83 ° 0. C16 H31 n 3 ° 2 64.52, H - 10.72, N - 14.29 64.61, H - 10.50, N - 14.13 oCHeHHH COCTaB: C -C - BHHHCJieHO , 264ΑβΗΟ, %%: 272 264 6 IIpHiiep 10. 2,2,6,6-TeTpaMeT5iJinMnepHAiiJiaMMflN-nznepzAMHonpo-ΠΜΟΗΟΒΟΜ KHCHOTEI (AT-34). Αηηλογμ ^ ηο npMMepy 6, H3 34.24 r (0.2 γ-μολ) μθτμ-ΠΟΒΟΓΟ 3 $ npa N -PΜΠθρΗΑΗΗΟΠρΟΠΗΟΗΟΒΟίί KMCJIOTH H 34.33 Γ (0.22 γ-μολ) ATAA nojiynaioT 29.3 r (49 , 6% ot TeopeTH-qeο-κογο, ΟΗΗΤΗΗ Ha ΜΘΤΚΛΟΒΗίί οφκρ -ΠΚΠβρΜΑΖΗΟΠροΠΗΟΗΟΒΟδkmcjiotn) iíejieBoro npoflyKTa c τ, πλ. 133-134 [deg.] C. < tb > 3 < tb > ______________________________________ < tb > ______________________________________ < tb > 0 -. H, 11.84; N, 14.63
Halen, %%: C - 69,10, H - 11,26, N - 14,22 11. Ροτοβητ κοΜπο3ζΐξΐιιο, cocToamym ks yflaponponHoro πο-HHCTjapojia c soSaBKOŽ 0,5 Mac.q. CTaČHJiHSaTopOB. PI 3 nojiy-ΗβΕΗΗΧ ΚΟΜΠΟβκυ, Ηβ ΓΟΤΟΒΗΤ 5% Q6H3 OJIbHBIM paCTBOp. IlOCJieποληογο pacTBopeHHH nojiKMepa h cTa6njiM3aTOpa b 6θη30λθμθτολομ nojiHBa Ha H, ejiJio $ aHOByK) nojmosney, orpaHHqeHHy © CTeKJIHHHHM KpyrOM, OTJIHBaiOT ΠΛ6ΗΚΖ. 4ΛΗ CpaBHeHMH ΓΟΤΟΒΗΤ aHanOrHqHLie Κ0ΜΠ03ΗΓξΗΜ C TH -HyBHHOM Π and τβκκθ ΠΛθΗκκ noHHMepa OES cTa6nHH3aTopa.IIojiyqeHHhie πλβηκμ τολπϊμηοΓι 70 mkm oÓJiywaKT ΗθφϋΛΒτροΒβΗ HHM-B yJIbTpaφHOJIeTOBδIM ΟΒΘΤΟΜ Ορβββ B03AyXa. B npoijecce cTapeHMH oTózpafflT προδΗ μ οπρβ, ξβΛΗωτ οτθ- neHb ΛθΟΤρνΚΙίΗΜ ΠΟΛΗΜθρβ ΜΘΤΟΑΟΜ ΜΚ-ΟΠβΚΤρΟΟΚΟΠΗΗ ΠΟ Ηθ- -1 κοπλθηηιο KapÓOHKHbHHX rpyiin Β οδΛβοτζ 1600-1800 ΗcoxpaHeHHK CM) κολμηθοτβθ aboííhiíx CBH3eíí b οΡληοτη 800-1000 CMB npopecce yΛbτpaφiIOΛeτoBOΓO oójryqeHWH.
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Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS852720A CS272264B1 (en) | 1985-04-12 | 1985-04-12 | Preparation of 2,2,6,6-tetramethylpiperidilamide carboxyl saturated acids |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS852720A CS272264B1 (en) | 1985-04-12 | 1985-04-12 | Preparation of 2,2,6,6-tetramethylpiperidilamide carboxyl saturated acids |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS272085A1 CS272085A1 (en) | 1988-02-15 |
| CS272264B1 true CS272264B1 (en) | 1991-01-15 |
Family
ID=5365093
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS852720A CS272264B1 (en) | 1985-04-12 | 1985-04-12 | Preparation of 2,2,6,6-tetramethylpiperidilamide carboxyl saturated acids |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS272264B1 (en) |
-
1985
- 1985-04-12 CS CS852720A patent/CS272264B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS272085A1 (en) | 1988-02-15 |
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